热处理温度对Co_(0.8)Fe_(2.2)O_4/SiO_2纳米复合薄膜结构和磁性能的影响

采用溶胶-凝胶旋涂法在经表面氧化的Si(100)基片上制备了Co0.8Fe2.2O4/Si O2纳米复合薄膜。利用X射线衍射仪、扫描电子显微镜和振动样品磁强计对Co0.8Fe2.2O4/Si O2纳米复合薄膜的结构、形貌和磁性能进行分析,研究了热处理温度对复合薄膜结构和磁性能的影响。结果表明:热处理温度高于750℃时复合薄膜中Co0.8Fe2.2O4呈现尖晶石结构;当热处理温度从750℃升高到1 100℃,复合薄膜中Co0.8Fe2.2O4的晶粒尺寸从6 nm增大到34 nm,晶胞常数从0.836 9 nm增大到0.839 5 nm。样品的矫顽力随热处理温度的升高先增大后减小,经1 000℃热处理样品的矫顽力达到298.3 k A/m。     

烧结温度对ZrO2薄膜表面形貌及力学性能的影响

采用溶胶-凝胶法在玻璃基体表面制备了经300℃,400℃和500℃烧结热处理的ZrO2薄膜.利用X射线衍射仪、原子力显微镜和纳米压痕仪研究了烧结温度对ZrO2薄膜表面形貌和力学性能的影响.实验结果表明,随着烧结温度的增加,ZrO2的晶体结构由少量的单斜晶相逐渐转变为单斜晶相和四方晶相的混合相.薄膜表面形貌逐渐改善,薄膜的表面粗糙度和颗粒度依次减小,薄膜的表面粗糙度分别为10.5 nm、7.2 nm和5.6 nm,ZrO2的粒径分别为188 nm、153 nm和130 nm.ZrO2薄膜的弹性模量和硬度都显著提高,薄膜的弹性模量分别为89.6 GPa、114.2 GPa和128.9 GPa,薄膜的硬度分别为7.6 GPa、10.3 GPa和15.1 GPa.     

烧结温度对不锈钢表面溶胶-凝胶ZrO2纳米薄膜摩擦学性能的影响

采用溶胶-凝胶法,在304不锈钢表面制备了分别经500℃、600℃和700℃下热处理的ZrO2薄膜.利用X射线衍射仪(XRD)、原子力显微镜(AFM)、扫描电镜(SEM)和摩擦磨损测试仪,研究了热处理温度对ZrO2薄膜的表面结构和摩擦学性能的影响.结果表明:随着温度的升高,ZrO2晶体结构逐渐由四方相(t-ZrO2)向单斜相(mZrO2)转变;当热处理温度从500℃升高到700℃时,ZrO2薄膜的平均晶粒度略有增大,但都在80 nm左右,晶粒分布趋于均匀致密,且其表面粗糙度由6.3 nm降低至4.6 nm左右.同时ZrO2薄膜的摩擦系数和磨损率分别从0.22和2.24×10-4mm3/Nm逐渐减小为0.19和1.95×10-4 mm3/Nm,因而薄膜的抗磨减摩性能也显著提高.     

TiO_2–ZnO复合薄膜的制备及光致双亲性能

采用溶胶-凝胶法制备了TiO2薄膜和ZnO掺杂的TiOr-ZnO复合薄膜.通过X射线衍射和原予力显微镜表征了样品的晶相、晶粒尺寸和形貌.以水(H2O)作为极性溶液参照物,苯(C6H6)作为非极性溶液参照物,研究了煅烧温度、煅烧时间、薄膜层数对薄膜光致双亲性的影响.结果表明:煅烧温度和煅烧时间的不同能够导致薄膜的晶粒粒径、晶型及薄膜表面的粗糙度发生变化.从页影响薄膜的双亲性能.当煅烧温度为550℃,煅烧时间 为2h,薄膜层数为3层时.TiO2由锐钛矿相向金红石转变,薄膜的双亲性最传.TiO2-ZnO复合薄膜的晶粒粒径约为25.2nm,薄膜表面粗糙度约1.815 nm,此时,亲水角和亲油角分别为5°和4°.ZnO掺杂的TiO2复合薄膜的双亲性明显高于纯TiO2薄膜.     

SnO2∶Sb/SiO2复合薄膜的制备与光学性能

采用溶胶-凝胶结合旋涂技术在玻璃基底上制备了SnO2∶Sb/SiO2复合薄膜,利用XRD、FT-IR、SEM、椭偏仪、分光光度计等方法对薄膜样品进行了系统地表征。结果表明:经过热处理后样品生成了SnO2∶Sb和SiO2;薄膜具有双层结构,上层SiO2厚度约105 nm,折射率为1.352,底层SnO2∶Sb厚度约1200 nm,折射率为1.91;优化工艺条件下SnO2∶Sb/SiO2复合薄膜的性能优于SnO2∶Sb薄膜,在相同情况下SnO2∶Sb/SiO2复合薄膜对可见光的透过率大于SnO2∶Sb薄膜,这是因为上层SiO2薄膜折射率较低,与底层高折射率SnO2∶Sb薄膜共同构成减反射膜系,提高了膜系的可见光透过率。相比于单层SnO2∶Sb膜,在可见光部分增透率大于4.5%,近红外波段的增透率小于1.0%,基本保持原有导电膜的低红外辐射特性,并提高了可见光透过率。     

有序介孔二氧化硅薄膜的制备及性能

以十六烷基三甲基溴化铵(CTAB)为模板剂,正硅酸乙酯为无机前驱体,在酸性条件下,采用溶胶-凝胶技术,用蒸发诱导自组装(EISA)工艺制备了二氧化硅透明介孔薄膜. 透射电子显微镜图显示热处理后的薄膜具有高度有序的六方相结构孔道;由椭偏仪测得热处理后薄膜的折射率低至1.18,厚度在180 nm左右;阻抗分析仪测得薄膜的介电常数为2.14. 薄膜经过六甲基二硅胺烷(HMDS)表面修饰后具有良好的疏水性能和热稳定性,作为低介电材料能更好满足工业需求.     

SiO2-MTES-CTAB-Al2O3纳米复合薄膜的制备及性能研究

以异丙醇铝和正硅酸乙酯为主要原料,采用溶胶-凝胶分步水解法,通过引入有机硅烷甲基三乙氧基硅烷和表面活性剂十六烷基三甲基溴化氨,并用乙二醇甲醚替换铝溶胶中水作为对比,制备了SiO2-MTES-CTAB-Al2O3纳米复合薄膜.通过FT-IR、可见光透射光谱分析、薄膜表面接触角测量及机械性能测试,研究了化学组成、煅烧温度和有无乙二醇甲醚替换对复合薄膜的影响.结果表明:不用乙二醇甲醚替换效果更好,经400 ℃热处理后不同配比复合薄膜在可见光区的透光率均大于85%,且不影响复合薄膜的疏水性,由于铝氧化物颗粒、十六烷基三甲基溴化氨和甲基三乙氧基硅烷的存在,所制备的纳米复合薄膜的硬度及耐摩擦性能均有较大提高,改善了力学性能,从而获得了具有良好的疏水性、透过率及硬质的SiO2-MTES-CTAB-Al2O3纳米复合薄膜.     

TiO2-SiO2/SiO2双层复合薄膜制备及折射率调控EI北大核心CSCD

采用溶胶-凝胶法制备了具有W型减反特性的Ti O2-SiO2/SiO2复合薄膜,并分别调控了TiO2及TiO2-SiO2混合介质薄膜折射率,探索了不同制备条件对TiO2薄膜折射率的影响机理。通过场发射扫描电子显微镜、能谱仪、椭偏仪、紫外–可见-红外分光光度计研究了薄膜微观结构、薄膜组分、折射率和光学透过率,通过TFcal软件模拟了双层复合薄膜的光学透过率线型。研究表明:溶胶pH值对TiO2薄膜折射率影响显著,其影响的前驱体水解速率对折射率的影响占主要作用,并且随着pH值的增大薄膜折射率减小,而水/钛比对薄膜折射率影响不显著。在TiO2与Si O2混合溶胶中两者物质的量比为1.2:1.0时,获得可用于制备双层复合W型减反膜系底层的薄膜,其椭偏仪拟合测试折射率约为1.68。最终制备的复合TiO2-SiO2/SiO2薄膜实现了光学宽谱范围380~1100 nm的优良增透效果,最大透过率可达约97%。     

TiO_2-SiO_2/SiO_2双层复合薄膜制备及折射率调控

采用溶胶-凝胶法制备了具有W型减反特性的Ti O_2-SiO_2/SiO_2复合薄膜,并分别调控了TiO_2及TiO_2-SiO_2混合介质薄膜折射率,探索了不同制备条件对TiO_2薄膜折射率的影响机理。通过场发射扫描电子显微镜、能谱仪、椭偏仪、紫外–可见-红外分光光度计研究了薄膜微观结构、薄膜组分、折射率和光学透过率,通过TFcal软件模拟了双层复合薄膜的光学透过率线型。研究表明:溶胶pH值对TiO_2薄膜折射率影响显著,其影响的前驱体水解速率对折射率的影响占主要作用,并且随着pH值的增大薄膜折射率减小,而水/钛比对薄膜折射率影响不显著。在TiO_2与Si O_2混合溶胶中两者物质的量比为1.2:1.0时,获得可用于制备双层复合W型减反膜系底层的薄膜,其椭偏仪拟合测试折射率约为1.68。最终制备的复合TiO_2-SiO_2/SiO_2薄膜实现了光学宽谱范围380～1100 nm的优良增透效果,最大透过率可达约97%。     

纳米二氧化钛薄膜的制备及性能研究

用溶胶-凝胶法在清洁的玻璃表面成功制备了均匀透明的纳米TiO2薄膜,并用X射线衍射仪,扫描电镜,红外光谱仪和接触角测定仪等对薄膜的结构和性质进行了研究.结果表明:薄膜由晶粒大小为20～45 nm的TiO2球型颗粒组成,膜表面均匀,结构致密,具有平整的组织结构;随热处理温度的增加,TiO2薄膜的晶相由无定型态转变成锐钛矿,最后在850℃热处理后完全转变成金红石相,且TiO2薄膜在经过紫外光的照射后亲水能力增强.     

Characterization of antireflective coatings on poly(methyl methacrylate) substrate by different process parameters

The high/low refractive index organic/inorganic antireflective (AR) hybrid polymers were formed using the sol–gel process, in which TiO₂/2‐hydroxyethyl methacrylate (2‐HEMA) (high refractive index hybrid polymer) and SiO₂/2‐HEMA (low refractive index hybrid polymer) two‐layer thin films were formed on a hard coating deposited poly(methyl methacrylate) (HC‐PMMA) substrate by both spin coating and dip coating. The relationship between the process parameters and the optical properties, thickness, porosity, surface morphology, and adhesion was determined. The results show that the reflectance of the two‐layer thin films on HC‐PMMA substrate is less than 0.21% (λ = 550 nm), with good adhesion (5B) and a hardness of up to 4H. In addition, the thickness, porosity, and roughness of the films affect refractive index and the antireflection properties of the AR two‐layered thin film. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Super black and ultrathin amorphous carbon film inspired by anti-reflection architecture in butterfly wing

An ultrathin and super black amorphous carbon (a-C) film has been fabricated by borrowing the inverse V-type anti-reflection nano-architecture from the black wings of butterfly Ornithoptera goliath through vacuum sintering process. The biomimetic a-C film shows good optical absorption (99%) at low reflectance (<1%) in visible light (380–795 nm), which is comparable to the previously fabricated darkest materials, while with a thickness (5 μm) of only 15% of those materials. Experimental results as well as theoretical simulation which is based on finite difference time domain method (FDTD) show that reflection of the fabricated inverse V-type structured a-C film is merely 1/13 of that of the flat surface a-C film, and 1/8 of that of glassy carbon. Complex refractive index of the derived a-C for visible light (380–795 nm) has also been calculated.     

氮化铝薄膜的光学性质

采用直流磁控溅射法在石英衬底上制备了氮化铝(AlN)薄膜.用X射线衍射仪分析了薄膜结构.利用椭圆偏振仪和紫外/可见/近红外分光光度计对AIN薄膜进行了相关光学性能的研究,获得到了薄膜的折射率随波长的色散关系曲线.在波长为250～1 000 nm,薄膜的折射率为1.87～2.20.结合透射光谱图,分析了AIN薄膜的光学性质.结果表明:利用磁控溅射方法可以获得(100)择优取向AIN薄膜;AIN薄膜在200～300 nm远紫外光范围内具有强烈的吸收,在300～1000 nm波长范围内具有良好的透过率.透射光谱图计算得到的薄膜厚度(427nm)与椭圆偏振拟合得到的薄膜厚度(425nm)一致.     

Surface plasmon resonance spectroscopic comparison of spiroxazine monolayer and polymeric thin film

Photochromic dye has recently attracted much interest in optical applications because of its reversible photoswitching properties by light irradiation. To apply those aspects of photochromism to actual photonic devices, the form of the thin film must be favorable to the photochromic molecular system. In this study, a polymeric thin film and self‐assembled monolayer were constructed with a photochromic spiroxazine derivative that is well known for its good fatigue properties. Their photoisomerization properties were characterized through surface plasmon resonance (SPR). As a result of ultraviolet irradiation to these thin films, the SPR angle shift clearly appeared as the optical thickness (Refractive index × Geometrical thickness) change in both of the films. The Fresnel calculation based on measurement results showed that the angle shift of the polymeric thin film mainly corresponded to the change of the refractive index. For the spiroxazine monolayer, the geometrical thickness change caused the resonance angle to shift dominantly. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 90: 3459–3465, 2003     

Modified Envelope Method for Obtaining Optical Properties of Weakly Absorbing Thin Films and Its Application to Thin Films of Pb(Zr,Ti)O3 Solid Solutions

A modified envelope method, which includes the consideration of the light intensity loss from the back surface of the substrate, was developed and shown to be a simple and convenient tool for obtaining the optical properties and the thickness of the film by using the transmission spectra alone in the medium and weak absorption regions. In the near-optical band gap region, both the transmission and the reflection spectra were used to calculate the optical constants of the films. This technique was applied to the thin films of PZT solid solutions across the entire composition range. The film thickness derived from the envelope method was cross-checked by a computer simulation method and was found to have an accuracy better than 2%. In addition, the refractive indices were fitted to a simple Sellmeier-type equation for determining the dispersion constants for PZT films. The valid wavelength range of these dispersion relations was from 350 to 2000 nm. The refractive index of the PZT films decreased linearly with increasing zirconium content. On the other hand, the optical band gap energy of the PZT films increased with increasing zirconium content.     

Synthesis and characterization of titanium dioxide optical films by sol–gel processes

The main purpose of this study is to synthesize the front panel of monitor with a high refractive index optical film. Our experiment uses titanium dioxide nanoparticles mixed with methyl methacrylate (MMA), 2‐hydroxyethyl methacrylate (2‐HEMA), and tri(ethylene glycol) dimethacrylate (TEGDMA) of the wet type and economical sol–gel production process. Our product has a superior mechanical, thermal, and optical properties was demonstrated by Fourier transform infrared spectrum (FTIR), differential scanning calorimeter (DSC), thermogravimetric analysis (TGA), UV/visible spectrum, and Spectro Ellipsometer. In addition, we found the surface of the two series of thin film with the organic and inorganic high refractive index (TiO₂) mixed materials, has high transmittance for visible light above 90%, refractive index <1.65 and the hardness test 6H. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 103: 2271–2280, 2007     

Optical and physical properties of zirconium dioxide reinforced poly(methyl methacrylate) nanocomposite films

The objective of this study was to investigate the fundamental aspects of acrylic resin and zirconia nanoparticle interaction to analyze the optical properties and subsequent changes in refractive index with incremental loading of nanoparticles. Poly(methyl methacrylate) (PMMA) reinforced with zirconia nanoparticles were prepared by dip coating, spin coating and solvent casting techniques. An overall understanding of the polymer nanocomposite film has been achieved using the spectroscopic and morphological studies. The vital aspect of this whole study is to derive a simple yet an efficient nanocomposite film capable of imparting extraordinary optical properties. Within the limitations of this research a very crucial property of the material has been revealed. The RI as well as the optical transparency of the nanocomposite film has been steadily maintained with a significant increase of RI by the magnitude of 0.06 and ~100% light transmittance on incorporation of pure zirconia nanoparticles into PMMA matrix has been achieved. The best technique found was spin coating as it could yield thin films and better transparency and higher refractive index.     

Research on Preparation,Structure and Properties of TiO2/Polythiourethane Hybrid Optical Films with High Refractive Index

Hybrid optical films of TiO₂‐triethoxysilane‐capped polythiourethane (TCPTU) with high refractive indices have been prepared via an in situ sol‐gel method. The high refractive index triethoxysilane‐capped polythiourethane (TCPTU) was synthesized by polyaddition of the triethoxysilane‐modified trimercaptothioethylamine (TMTEA) and 2,2′‐dimercaptoethylsulfide (MES) with 2,4‐tolylene diisocyanate (TDI). The titania content in the hybrid films can be adjusted from 0 to 80 wt.‐% by the feed ratio of titania precursor [Ti(OBu)₄] to polymer (TCPTU). Both FTIR and DSC analyses indicate that there is chemical bonding between the titania domain and the polymer chain. TGA results suggest that the titania of high content was successfully incorporated into polymer matrices and this series of hybrid films have good thermal properties. AFM measurements indicate that in the hybrid films the titania domains are of nanosize scale and the domain size averagely decreases from 60–80 nm to 5–20 nm with increasing content of titania, and the variation of surface roughness for the hybrid films has the same trend. These may be relative to the content of TCPTU and the interaction between titania and polymer (TCPTU). The refractive indices of the hybrid films at 632.8 nm increased from 1 632 to 1 879 as the titania content varied from 0 to 80 wt.‐%.

AFM image of the hybrid film.     

Nanostructured titanium nitride for highly sensitive localized surface plasmon resonance biosensing

Titanium nitride (TiN) as an alternative plasmonic ceramic material with superb properties including high hardness, outstanding corrosion resistance and excellent biocompatibility, has exhibited great potential for optical biochemical sensing applications. By sputtering about 35 nm–50 nm TiN on glass (f-TiN), the surface was found to provide sensing capability toward NaCl solution through the phenomenon of surface plasmon resonance. When the TiN film of about 27 nm–50 nm in thickness was sputtered onto a roughened glass surface (R–TiN), the sensing capability was improved. This was further improved when holes at nanoscale were created in the TiN film of about 19 nm–27 nm in thickness (NH–TiN). The roughened surface and nanohole patterns provided confinement of surface plasmons and significantly improved the sensitivity toward the local refractive index changes. In detail, the calculated refractive index resolution (RIR) of the optimal NH–TiN sensors for NaCl was found to be 9.5 × 10⁻⁸ refractive index unit (RIU), which had outperformed the f-TiN and R–TiN sensors. For biosensing, the optimized NH–TiN sensor was found to be capable to detect both small and large biomolecules, i.e. biotin (molecular weight of 244.3 g/mol) and human IgG (160,000 g/mol), in a label-free manner. Especially, the NH–TiN sensor significantly improved sensitivity in detecting small molecules due to the localized plasmonic confinement of electromagnetic field. Combining with the excellent mechanical and durability properties of TiN, the proposed NH–TiN can be a strong candidate for plasmonic biosensing applications.     

Photoinduced reversible refractive index changes in doped poly(methyl methacrylate) lightguides

Planar polymer lightguides of poly(methyl methacrylate)(PMMA) doped with the azo dye, N,N-dihexyl-4-amino-4′-nitro-azobenzene (DHANA) were fabricated on a suitable glass substrate or on one surface of a regular prism. The absorption of this azo dye is strong in the green spectral region. With the red light of a HeNe laser (633 nm) these polymer films may be used as lightguides. However, in this spectral region, the guided light influences the waveguiding properties of the polymer film, making this combination a possible candidate for an all optical device material. The observed refractive index changes are intensity dependent and the response time is of the order of 100ms.